HRID1054005

反应详情

EQUATION

反应方程式

HRID 1054005 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture containing 47 (1.0 g, 2.3 mmol) and 10% Pd-on-carbon (˜1 g) in anhydrous MeOH (20 mL) was placed under a hydrogen atmosphere (45 PSI) and shaken using a Parr apparatus for 1 h. The catalyst was removed by filtration and the solids were washed with EtOAc and MeOH. The clarified filtrate was concentrated to afford 634 mg (91%) of 48 as an orange oil which was used without further purification. 1H NMR (CDCl3, 300 MHz) δ7.51-7.49 (m, 1H), 7.38-7.35 (m, 1H), 7.21-7.17 (m, 2H), 4.16-4.09 (m, 2H), 3.68-3.59 (m, 2H), 3.12-3.07 (m, 2H), 2.88-2.73 (m, 4H), 1.84-1.69 (m, 4H), 1.43-1.39 (m, 1H), 1.26-1.20 (m, 3H) ppm.

WORKUP

后处理

  1. customfor 1 h
  2. customThe catalyst was removed by filtration
  3. washthe solids were washed with EtOAc and MeOH
  4. concentrationThe clarified filtrate was concentrated